目的 探索利用改进PM2.5中16种多环芳烃高效液相色谱法测定合肥市大气细颗粒物PM2.5中多环芳烃含量。方法 取采集空气后滤膜1/4剪碎,乙腈超声提取,高效液相色谱法测定,改用多环芳烃( Polycyclic aromatic hydrocarbons,PAHs)专用柱(4.60 mm×250 mm,5.0 μm),流动相为水和乙腈,流速1.5 mL/min,梯度洗脱,PDA检测器和FLR检测器同时检测。结果 16种PAHs空白加标回收率在72%~105%之间,标准曲线线性方程相关系数r>0.999,相对标准差(RSD) 0.61%~7.72%,方法检出限为0.004~0.023 ng/m3,定量下限为0.014~0.094 ng/m3(采样量为144 m3)。结论 改进过后的方法在检测合肥市大气颗粒物PM2.5中具有简便、快速、灵敏等优点,提高了低环数PAHs回收率和PAHs分离效果,具有较高的应用价值。
Abstract
Objective To develop an improved high performance liquid chromatography(HPLC) method for the determination of 16 kinds of polycyclic aromatic hydrocarbons(PAHs) in PM2.5 in Hefei. Methods After collecting air,1/4 of filter membrane was cut up,acetonitrile was added for ultrasonic extraction,and determined by HPLC method.The special column for PAHs (4.60mm × 250mm,5.0 μ m) was used,the mobile phase was water and acetonitrile,the flow rate was 1.5ml/min,gradient elution method was used,PDA detector and FLR detector were detected at the same time. Results The blank spike recovery rates of 16 kinds of PAHs ranged from 72%~105%.The correlation coefficient of linear equation of standard curve was r>0.999.The relative standard deviation (RSD) was 0.61%~7.72%.The detection limit was 0.004~0.023ng/m3,and the lower limit of quantification was 0.014~0.094ng/m3 (sampling volume was 144 m3). Conclusion The improved method has the advantages of simplicity,rapidity and sensitivity in the detection of PM2.5 in the atmosphere.It improves the recovery rate of PAHs with low ring number and the separation effect of PAHs,and has high application value.
关键词
大气 /
细颗粒物PM2.5 /
多环芳烃 /
超声萃取 /
超高效液相色谱
Key words
Atmosphere /
Fine Particulate Matter PM2.5 /
PAHs /
Ultrasonic extraction /
Ultra performance liquid chromatography (UPLC)
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参考文献
[1] 张秀蓝,任立军,杨文龙,等.液相色谱法测定大气样品中多环芳烃的方法优化[J].环境化学,2017,36(3):621.
[2] 殷婧,夏忠欢,周彦池,等.临汾市售蔬菜中多环芳烃污染特征及致癌风险分析[J].生态毒理学报,2016,11(3):265.
[3] Barco-Bonilla N,Martinez Vidal JL,Garrido A,et al.Comparison of ultrasonic and pressurized liquid extraction for the analysis of polycyclic aromatic compounds in soil samples by gas chromatography coupled to tandem massspectrometry[J].Talanta,2009,78(1):156-164.
[4] Barco-Bonilla N,Romerro-Gonzalez R,Plaza-Bolanos P,et al.Comprehensive analysys of polycyclic aromatic hydrocarbons in wastewater using stir bar sorptive extraction and gas chromalography coupled to landem mass spectrometry[J].Anal Chim Acta,2011,693(1):62-71.
[5] Wenzl T,Simon R,Anklam E,et al.Analytical methods for polycyclic aromatic hydrocarbons (PAHs) in food and the environment needed for new food legislation in the European Union[J].Trend Anal Chem,2006,25(7):716-725.
[6] Nording M,Frech K,Perssion Y,et al.On the semi-quantification of polycyclic aromatic hydrocarbons in contaminated soil by an enzyme-linked immunosorbent assay kit[J].Anal ChimActa,2006,555(1):107-113.
[7] 邓晓燕,张大海,李先国.气相色谱法测ta定水体中多环芳烃的前处理方法优化[J].分析试验室,2015,34(5):525.
[8] 徐媛,刘文民,赵景红,等.固相萃取搅拌棒萃取-气相色谱分析海水中的多环芳烃[J].分析化学,2005,33(10):1401.
[9] 祝本琼,陈浩,李胜清.基于轻质萃取剂的溶剂去乳化分散液-液微萃取-气相色谱法测定水样中多环芳烃[J].色谱,2012,30(2):201.
[10] 陈月萌,赵敏,王千,等.毛细管气相色谱法测定工作场所空气中3种多环芳烃[J].理化检验(化学分册),2014,50(11):1409.
[11] 王美飞,杨丽莉,胡恩宇.微波提取-高效液相色谱法测定大气颗粒物中的多环芳烃[J].色谱,2017,35(6):669.
[12] 李建平,渠志华,王辰.等,大气颗粒物PM2.5中16种多环芳烃的超高效液相色谱测定法[J].环境与健康杂志,2017,34(2):164.
[13] 高娟,郭伟杰,刘娜,等.硫酸酸化-气相色谱-质谱法测定植物提取物中的4种多环芳烃[J].理化检验(化学分册)),2017,53(6):684.
[14] 冯利,张胜军,朱国华,等.大体积搅拌棒吸附萃取技术与热脱附-气相色谱-质谱法测定地表水中多环芳烃[J].色谱,2017,35(4):466.
[15] 司晓喜,朱瑞芝,张凤梅,等.多次溶剂萃取-气相色谱/串联质谱法测定热熔胶中的多环芳烃[J].分析化学,2016(3):430.
[16] Guilherme M,Titato,Fernando M,et al.Optimization and Validation of HPLC-UV-DAD and HPLC-APCI-MS Methodologies for the Determination of Selected PAHs in Water Samples[J].J Chromatogr Sci,2006,44(2):35-40.
[17] Liao C,Yang P,Zhenwei Xi ZW,et al.Application of GC–Triple Quadrupole MS in the Quantitative Confirmation of Polycyclic Aromatic Hydrocarbons and Phthalic Acid Esters in Soil[J].J Chromatogr Sci,2010,48(3):161-166.
[18] Rocha,M,Ferreira PC,A.Reis,et al.Determination of Polycyclic Aromatic Hydrocarbons in Coastal Sediments from the Porto Region (Portugal) by Microwave-Assisted Extraction,Followed by SPME and GC-MS[J].J Chromatogr Sci,2011,49(10):695-701.
[19] Cam D,Gagni S,L.Meldolesi L,et al.Determination of Polycyclic Aromatic Hydrocarbons in Sediment Using Solid-Phase Microextraction with Gas Chromatography–Mass Spectrometry[J].J Chromatogr Sci,2000,38(2):55-60.
[20] M.O.Punín Crespo1,D.Cam,S.Gagni,et al.Extraction of Hydrocarbons from Seaweed Samples Using Sonication and Microwave-Assisted Extraction: A Comparative Study[J].J Chromatogr Sci,44(11):615-618.
[21] 李静静,李云飞,谢继锋,等.中空纤维膜液相微萃取与GC-MS联用测定地表径流中的多环芳烃[J].环境化学,2013,23(11):2170-2175.
[22] 王超,彭涛,吕怡兵,等.液相色谱法测定水中16种多环芳烃的方法优化[J].环境化学,2014,33(1):62.
[23] 夏世钧,多环芳烃对人类环境的污染、致癌作用及其预防[J].国外医学参考资料(卫生学分册),1974,3,79-91.
[24] 许云竹,花修艺,董德明,等.地表水环境中PAHs源解析的方法比较及应用[J].《吉林大学学报(理学版)》,2011,49 (3):565-574.
基金
1.中央财政资金补助雾霾监测专项;2.合肥市医学重点学科建设资助
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